US8418535B2 - Method and apparatus for integrated measurement of the mass and surface charge of discrete microparticles using a suspended microchannel resonator - Google Patents
Method and apparatus for integrated measurement of the mass and surface charge of discrete microparticles using a suspended microchannel resonator Download PDFInfo
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- US8418535B2 US8418535B2 US12/799,922 US79992210A US8418535B2 US 8418535 B2 US8418535 B2 US 8418535B2 US 79992210 A US79992210 A US 79992210A US 8418535 B2 US8418535 B2 US 8418535B2
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N29/00—Investigating or analysing materials by the use of ultrasonic, sonic or infrasonic waves; Visualisation of the interior of objects by transmitting ultrasonic or sonic waves through the object
- G01N29/02—Analysing fluids
- G01N29/036—Analysing fluids by measuring frequency or resonance of acoustic waves
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N2291/00—Indexing codes associated with group G01N29/00
- G01N2291/02—Indexing codes associated with the analysed material
- G01N2291/024—Mixtures
- G01N2291/02408—Solids in gases, e.g. particle suspensions
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N2291/00—Indexing codes associated with group G01N29/00
- G01N2291/02—Indexing codes associated with the analysed material
- G01N2291/028—Material parameters
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
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- G01N2291/028—Material parameters
- G01N2291/02863—Electric or magnetic parameters
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N5/00—Analysing materials by weighing, e.g. weighing small particles separated from a gas or liquid
Definitions
- This invention is based on a published work by the inventors: “Integrated Measurement of the Mass and Surface Charge of Discrete Microparticles Using a Suspended Microchannel Resonator;” Philip Dextras, Thomas P. Burg and Scott R. Manalis; Anal. Chem ., 2009, 81 (11), pp 4517-4523; Publication Date (Web): May 8, 2009 (Article); DOI: 10.1021/ac9005149. The contents of this article are incorporated in their entirety by reference.
- the invention relates to utilizing the high-resolution particle measurement capabilities of a Suspended Miccrochannel (SMR) resonator in combination with an applied oscillating electric field to provide an unprecedented single particle characterization capability
- SMR Suspended Miccrochannel
- Colloidal dispersions have a broad range of technological applications, including paints, pharmaceuticals, foods, photographic emulsions, ceramics, drilling muds, inks, and photonic crystals. Many of these applications require very precise control over colloidal stability and hence inter-particle interactions which are dependent on the physico-chemical properties of the particles themselves. Quantitative measures of particle properties such as the size, mass and surface charge are therefore often of value in designing systems and manufacturing processes for these applications. Measurements of particle size and surface charge are routinely performed using light scattering techniques such as phase analysis light scattering (PALS). This technique estimates the size and electrophoretic mobility of particles by measuring their average Brownian motion and their motion in an applied electric field respectively.
- PALS phase analysis light scattering
- PALS While applicable to a wide variety of colloidal systems, PALS reports size and mobility values which represent averages over multiple particles. Hence accuracy in estimating the particle's charge, which is dependent on both the size and the mobility, can suffer from errors made in ensemble average measurements of these two parameters, both of which may be multi-modal for a complex population.
- Carbon nanotube-based Coulter counters are able to measure discrete-particle mobility and size, but compromises must be made between the signal-to-noise ratio (SNR) of the mobility measurement and that of the size measurement since they have inherently different optimum orifice lengths.
- SNR signal-to-noise ratio
- Measurement of particle charge-to-mass ratio by time-of-flight mass spectrometry has been integrated with direct charge measurement using a Faraday disc, but because the sample must be dried, the measured charge may not accurately reflect that experienced in the desired dispersion medium for a given application.
- SMR particle detection and measurement based on the use of SMR's
- the SMR uses a fluidic microchannel embedded in a resonant structure, typically in the form of a cantilever or torsional structure. Fluids, usually containing target particles are flowed through the sensor, and the contribution of the flowed material to the total mass within the sensor causes the resonance frequency of the sensor to change in a measurable fashion.
- SMR's are typically microfabricated MEMS devices. The use of microfabricated resonant mass sensors to measure fluid density has been known in the literature for some time [P. Enoksson, G. Stemme, E.
- This resolution is sufficient to detect and measure the mass of individual particles in the range of ⁇ 100 nanometers up to many microns in size, including mammalian cells.
- the resonance frequency of the SMR is highly sensitive to its position along the SMR channel.
- SMR based techniques overcome some of the disadvantages of the prior art in terms of individual particle characterization, it would be desirable to utilize the measurement capabilities of an SMR to finely characterize mass and position and extend the range of particle characterization.
- the invention is a Suspended Microchannel Resonator (SMR) system including a resonant structure with at least one fluid channel whose surfaces contacting the fluid are electrically insulating, an oscillating voltage source whose electrodes are disposed to produce an oscillating electric field in the fluid across the channel length, and an actuator for oscillating the resonant structure mechanically coupled to the structure whose drive means is electrically isolated from the oscillating electric field, the fluid channel and any part of the SMR structure.
- SMR Suspended Microchannel Resonator
- the electrically insulating surfaces may be a thermal oxide passivation layer grown on the bulk resonant structure.
- the invention is a method for measuring surface charge of a target particle including the steps of
- the invention may include measuring the particle mass and density by previously disclosed SMR measurements. With the above steps performed, sufficient information is available for calculating the particle surface charge.
- FIG. 1 is a schematic illustration of SMR resonant behavior when a particle flows through the channel.
- FIG. 2 depicts SMR resonant behavior when a particle flowing through it is subject to an oscillating electric field.
- FIG. 3 depicts an SMR configured with an inner channel surface insulating layer.
- FIG. 4 depicts an SMR driven by an external actuator as opposed to the typical integrated actuators used by current devices.
- FIG. 5 is a block diagram of an implemented control system and SMR set-up
- an observed shift in SMR resonant frequency is dependent on the particle's position in the channel.
- the resonant shift is greatest when the particle is in the area nearest the end of the cantilever.
- the resonant shift follows a curve like the idealized curve shown in the figure.
- FIG. 2 if an oscillating voltage source 4 is placed in the system, such that the particle 3 experiences a suitably powerful oscillating electric field as it traverses SMR channel 2 , due to electrophoretic and electro-osmotic effects, the particles course will be modulated producing an SMR frequency shift similar to the idealized curve shown in the Figure.
- improvements to the SMR set-up and measurement protocols were found important to achieving useful results.
- SMR's of the type described herein are microfabricated MEMS devices, necessarily so to achieve the small scale and physical characteristics required for femtogram resolution. Thus necessarily the substrate materials tend to be at least partly conductive. In order to support an electric field in the fluid-filled channel, the channel needs to be electrically insulated. For a MEMS type device, a convenient way to accomplish this, as shown in FIG. 3 , is to grow a passivation layer 5 on the interior walls of channel 2 . In the case of a suitable SMR actually tested by the inventors, the base SMR was fabricated from silicon. In the exemplary SMR, electrical passivation of the device was accomplished by growing 800 ⁇ of thermal oxide on all silicon surfaces contacting the fluid. Dry thermal oxide was grown at 850° C.
- This oxide has been found to support electric fields up to 1650 V/cm in the fluid before it breaks down and shunts current through the bulk silicon.
- the SMR is driven into oscillation by actuation means integrated into the SMR substrate, such as the substrate being one electrode of a piezo-resistive or electrostatic actuation scheme, as are well known in the related art of Atomic Force Microscopy (AFM) for AFM cantilever actuation.
- AFM Atomic Force Microscopy
- This approach is convenient because the actuation can be built into the SMR as part of the microfabrication process.
- the SMR contains a microchannel, using the SMR substrate as an electrode in the drive circuit creates a large ground plane behind the walls of this microchannel which is separated from the fluid by only the passivation oxide thickness, or some similar thin layer.
- an external actuator 7 to drive SMR 1 whose drive means is not part of any circuit including the channel, fluid, and the substrate, is a preferable approach.
- actuation was performed by means of a piezoelectric crystal external to the device (PL022, Physik Instrumente GmbH & Co.
- This crystal's 4 mm 2 footprint is small enough that it can make direct contact with the device's 145 mm 2 bottom surface without interfering with the optical lever beam.
- Contact force is adjusted by means of a set screw embedded in the manifold which seals external tubing against the device's fluid access ports on its top surface. No electrical circuit interaction exists between the piezo drive, the substrate, and the channel voltage circuit.
- Electrodes for electrophoresis were also integrated at the system level in order to minimize complications due to electrolysis. This was accomplished using a custom manifold incorporating both platinum wire electrodes and air pressure control elements needed to achieve precise control over the particle drift velocity.
- a schematic of the exemplary system is shown in FIG. 5 .
- the surface charge of a particle may be calculated from the zeta-potential of the particle and the physical dimensions of the particle.
- the physical dimensions can be derived from previously disclosed techniques available from a suitable SMR, such as utilized by the present invention, improved as disclosed for the particular set-up involving an applied oscillating electric field.
- the zeta potential can be calculated in a system such as shown in FIG. 2 if the electric field is known, the local amplitude of oscillation due to electrophoretic and electro-osmotic flow is known, and if the channel wall zeta-potential is known.
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- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Investigating Or Analyzing Materials By The Use Of Electric Means (AREA)
Abstract
Description
-
- 1. flowing the target particle in a fluid through the fluid channel of a resonating Suspended Micro Channel Resonator (SMR),
- 2. applying an oscillating voltage in the fluid across the length of the fluid channel,
- 3. determining the local oscillating E-field developed by the oscillating voltage for positions along the channel,
- 4. determining the zeta-potential of the fluid channel walls,
- 5. measuring the shift in SMR resonance and determining the local amplitude of particle oscillation due to elecrtrophoretic and electro-osmotic motion of the particle caused by the oscillating E-field from the resonant shift,
- 6. calculating the particle zeta-potential from the E-field, channel wall zeta-potential, and oscillation amplitude
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Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
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US10234444B2 (en) | 2015-09-29 | 2019-03-19 | The Board Of Trustees Of The University Of Illinois | System and method for nano-opto-mechanical-fluidic sensing of particles |
US11346755B2 (en) | 2019-01-10 | 2022-05-31 | Travera, Inc. | Calibration of a functional biomarker instrument |
US11530974B1 (en) | 2021-11-01 | 2022-12-20 | Travera, Inc. | Cellular measurement, calibration, and classification |
Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US5417104A (en) * | 1993-05-28 | 1995-05-23 | Gas Research Institute | Determination of permeability of porous media by streaming potential and electro-osmotic coefficients |
US7780842B2 (en) * | 2004-06-11 | 2010-08-24 | Carnegie Mellon University | Apparatus and method for determining the zeta potential of surfaces for the measurement of streaming metrics related thereto |
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Patent Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
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US5417104A (en) * | 1993-05-28 | 1995-05-23 | Gas Research Institute | Determination of permeability of porous media by streaming potential and electro-osmotic coefficients |
US7780842B2 (en) * | 2004-06-11 | 2010-08-24 | Carnegie Mellon University | Apparatus and method for determining the zeta potential of surfaces for the measurement of streaming metrics related thereto |
Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US10234444B2 (en) | 2015-09-29 | 2019-03-19 | The Board Of Trustees Of The University Of Illinois | System and method for nano-opto-mechanical-fluidic sensing of particles |
US11346755B2 (en) | 2019-01-10 | 2022-05-31 | Travera, Inc. | Calibration of a functional biomarker instrument |
US11530974B1 (en) | 2021-11-01 | 2022-12-20 | Travera, Inc. | Cellular measurement, calibration, and classification |
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US20110271747A1 (en) | 2011-11-10 |
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